CN103510092B - Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof - Google Patents
Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof Download PDFInfo
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- CN103510092B CN103510092B CN201210204195.2A CN201210204195A CN103510092B CN 103510092 B CN103510092 B CN 103510092B CN 201210204195 A CN201210204195 A CN 201210204195A CN 103510092 B CN103510092 B CN 103510092B
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- 238000009749 continuous casting Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- 239000003518 caustics Substances 0.000 title abstract 2
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 14
- -1 sodium alkyl benzene Chemical class 0.000 claims abstract description 14
- 230000007547 defect Effects 0.000 claims abstract description 12
- 229940077388 benzenesulfonate Drugs 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 3
- 229950002929 trinitrophenol Drugs 0.000 claims description 28
- 229910000831 Steel Inorganic materials 0.000 claims description 24
- 239000010959 steel Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 2
- 229940075930 picrate Drugs 0.000 claims description 2
- OXNIZHLAWKMVMX-UHFFFAOYSA-M picrate anion Chemical compound [O-]C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-M 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 16
- 230000007797 corrosion Effects 0.000 abstract description 16
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 6
- 239000010955 niobium Substances 0.000 abstract description 5
- 239000010936 titanium Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 4
- 229910052758 niobium Inorganic materials 0.000 abstract description 3
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052720 vanadium Inorganic materials 0.000 abstract description 2
- 229910000742 Microalloyed steel Inorganic materials 0.000 abstract 1
- 238000004134 energy conservation Methods 0.000 abstract 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 16
- 238000005530 etching Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a corrosive agent for displaying intercrystalline crack defects in a continuous casting billet, which comprises the following chemical components: 3-4 g of picric acid; 10-20 ml of sodium alkyl benzene sulfonate; 500-800 ml of absolute ethyl alcohol; 150-300 ml of hydrochloric acid and 40-60 ml of nitric acid, and the preparation method comprises the steps of putting a quantitative picric acid solid medicament into a glass container, taking 2000ml of distilled water, dividing the distilled water into two parts, adding one part of distilled water into the picric acid solid medicament, adding absolute ethyl alcohol into a picric acid aqueous solution, and adding hydrochloric acid into the solution; adding a specified amount of nitric acid into the standby distilled water, pouring the nitric acid aqueous solution into the aqueous solution of the picric acid and hydrochloric acid medicament, mixing, uniformly stirring, finally pouring a certain amount of sodium alkyl benzene sulfonate into the prepared solution, and fully stirring. The invention has the characteristics of safety, reliability, easy storage, high corrosion speed, little pollution, energy conservation, simple and convenient operation and the like, and is used for silicon steel; the niobium, vanadium and titanium microalloyed steel has wide applicability.
Description
Technical field
Patent of the present invention relates to metallurgical analysis zone material inspection field, particularly a kind of mordant for showing continuous casting steel billet intercrystalline crack and compound method thereof.
Background technology
The macrostructure fault detection method of continuous casting steel billet mainly contains hot aciding, cold aciding, sulfur print test method, dendrite etch.These methods demonstrate its feature in actual applications separately, hot aciding corrosive power is strong, for showing the macrostructure defect of steel, owing to being that strong acid aqueous solution is heated corrosion, defect is exposed complete, but tiny defect edge etch fall by another effect of deep-etching exactly, crackle alligatoring, expanded configuration is destroyed, and acid mist produces severe contamination to environment.Therefore not good to the display effect of continuous casting steel billet intercrystalline crack, particularly On Crack Propagation trend can not completely be reproduced.The segregation form of sulphur in sulfur print test method reflection steel, to low-sulfur steel, acid etching effect is visible hardly.Cold acid etching method of inspection pollutes little, easy to operate, meets low-carbon environment-friendly theory, is therefore used widely, check with alternative hot acid.But current cold acid etching reagent is all conventional macrostructure and the defect of display steel, does not prove effective to intercrystalline crack.Dendrite method of inspection belongs to cold acid etching category, but shown be the arborescent structure form formed in the process of setting of steel.This comparatively microscopic defect of low power intercrystalline crack is mainly formed along low power grain boundary, and therefore dendrite etch has certain limitation.
Some are contained to the continuous casting steel billet of Nb, Ti microalloying, when curing condition fluctuation is larger, often easily formed along brilliant pattern cracking defect at the columnar zone of continuous casting steel billet, this crackle is tiny, tortuous, be difficult to fully manifest by routine inspection method, but can produce the follow-up rolling of strand and have a strong impact on, be easy to make steel billet produce transverse breakage, therefore, in order to original appearance shows form, distribution characteristics, the expansion trend of this intercrystalline crack, study its harmfulness, be necessary the cold acid corrosion agent of developing a kind of effective display continuous casting steel billet intercrystalline crack defect.
Summary of the invention
The present invention is a kind of mordant for showing continuous casting steel billet grain-boundary crack and compound method thereof, is a kind of cold acid etching method of available property corrosion, can original appearance display continuous casting steel billet intercrystalline crack, expanded configuration.Solve with the methods such as general acid etching can not the continuous casting steel billet columnar zone such as complete clear display silicon steel, the display of triangle crystalline region intergranular microcrack form problem.
The present invention is formulated by picric acid, sodium alkyl benzene sulfonate, absolute ethyl alcohol, hydrochloric acid, nitric acid, distilled water, and its every part proportioning share is as follows:
Picric acid (trinitrophenol) C
6h
3n
3o
73-4 grams
Sodium alkyl benzene sulfonate R-C
6h
4-SO
3na 10-20 milliliters
Absolute ethyl alcohol C
2h
5oH (mass percent: 99.8%) 500-800 milliliters
Hydrochloric acid HCl (mass percent: 36%) 150-300 milliliters
Nitric acid HNO
3(mass percent: 63.8%)
40-60 milliliters
Distilled water 2000 milliliters.
Compound method of the present invention is as follows:
Quantitative picric acid solid chemicals is placed in a glass container by ormal weight, gets distilled water 2000 milliliters, be divided into two parts, portion joins in picric acid solid chemicals, and another part for subsequent use.The absolute ethyl alcohol getting ormal weight joins in picric acid aqueous solution, then is joined in picric acid ethanol water by quantitative hydrochloric acid.The nitric acid separately getting ormal weight joins in distilled water for subsequent use.Again aqueous solution of nitric acid is poured in the aqueous solution of picrate acid treatment and mix, uniform stirring, finally quantitative sodium alkyl benzene sulfonate is poured in the solution previously prepared, fully stir.Complete the preparation of reagent, can use.
The principal ingredient that the present invention is mordant with hydrochloric acid, nitric acid, will according to the content of picric acid and sodium alkyl benzene sulfonate in carbon in steel and micro alloying element content adjustment formula during preparation, when carbon content height, suitable increase picric acid amount, meanwhile, sodium alkyl benzene sulfonate amount is increased matchingly, when sodium alkyl benzene sulfonate addition is too much, the chemical reaction of other component medicament will be suppressed, mordant was lost efficacy.
The beneficial effect that mordant of the present invention corrodes continuous casting steel billet low power intercrystalline crack defect is utilized to be: except can showing the conventional macrostructure defects such as continuous casting steel billet center segregation, center porosity, manifest along the brilliant crack defect original appearance formed in continuous casting steel billet columnar zone, triangle crystalline region, fracture edges does not expand, and does not reduce.Particularly crack tip expanded configuration is clear, complete to the fragility Edge crystal crack form display that silicon steel continuous strand presents,
Mordant of the present invention belongs to weak cold acid etching reagent, the matrix form in macrostructure can be suppressed, the display of strengthening crystal boundary, the corrosion contaminant formed is few, avoid due to hot acid erosion, sufur printing corrode cause intercrystalline crack coarse language, crack tip passivation, many character that is unfavorable for judging ftractureing such as fuzzy corrosive effect, for differentiating crack-type, infer that casting blank cleavage reason provides full and accurate tangible evidence.
The cold acid corrosion agent of low power of the present invention has safety, reliably, is easy to deposit, and the features such as corrosion speed is fast, pollutes little, economize energy, easy and simple to handle, to silicon steel; Niobium, vanadium, titanium microalloying steel have applicability widely.
Embodiment
Content of the present invention is described in detail below by several specific embodiment.
Embodiment 1
For display containing C 0.04%; Si 1.45; Mn 0.65%; Cr 0.033%; Nb 0.01%; The silicon steel continuous strand intercrystalline crack form of Ti 0.015%.
Get 3 grams of picric acid, join in 1000 ml distilled waters, get 500 milliliters of absolute ethyl alcohols and join in picric acid aqueous solution, then get 150 milliliters of hydrochloric acid and join in picric acid absolute ethyl alcohol aqueous solution.Separately get distilled water 1000 milliliters, add 40 milliliters of nitric acid, aqueous solution of nitric acid is slowly poured in picric acid absolute ethyl alcohol aqueous hydrochloric acid solution and mix.Get 20 milliliters of sodium alkyl benzene sulfonates to join in the appearance agent mixed, fully stir, form cold acid etching corrosion liquid 1 of the present invention.
Dip in corrosion liquid 1 wiping specimen surface with absorbent cotton, uniform corrosion 3-5 minute, the grain boundaries crack form on the examination face of being observed visually to manifest when knowing immediately to examination face upper punch hot water or cold water, dries up.
Embodiment 2
For display containing C 0.0026%; Si 1.26%; Mn 0.52%; Cr 0.015%; Nb 0.004%;
Ti 0.016%; The silicon steel continuous strand intercrystalline crack form of V0.004%.
Get 4 grams of picric acid, join in 1000 ml distilled waters, get 600 milliliters of absolute ethyl alcohols and join in picric acid aqueous solution, then get 180 milliliters of salt and join in picric acid absolute ethyl alcohol aqueous solution.Separately get distilled water 1000 milliliters, add 50 milliliters of nitric acid, aqueous solution of nitric acid is slowly poured in picric acid absolute ethyl alcohol aqueous hydrochloric acid solution and mix.Get 20 milliliters of sodium alkyl benzene sulfonates to join in the appearance agent mixed, fully stir, form cold acid etching corrosion liquid 2 of the present invention.
Dip in corrosion liquid 2 wiping specimen surface with absorbent cotton, uniform corrosion 3-5 minute, the grain boundaries crack form on the examination face of being observed visually to manifest when knowing immediately to examination face upper punch hot water or cold water, dries up.
Embodiment 3
For display containing C 0.003%; Si 0.03-0.05%; Mn 0.18%; The Hi-Stren steel continuous casting billet intercrystalline crack form of Ti0.1%.
Get 4 grams of picric acid, join in 1000 ml distilled waters, get 800 milliliters of absolute ethyl alcohols and join in picric acid aqueous solution, then get 200 milliliters of salt and join in picric acid absolute ethyl alcohol aqueous solution.Separately get distilled water 1000 milliliters, add 60 milliliters of nitric acid, aqueous solution of nitric acid is slowly poured in picric acid absolute ethyl alcohol aqueous hydrochloric acid solution and mix.Get 20 milliliters of sodium alkyl benzene sulfonates to join in the appearance agent mixed, fully stir, form cold acid etching corrosion liquid 3 of the present invention.
Dip in corrosion liquid 3 wiping specimen surface with absorbent cotton, uniform corrosion 5-7 minute, the grain boundaries crack form on the examination face of being observed visually manifests when knowing, immediately to examination face upper punch hot water or cold water, dries up.
Claims (2)
1. show a mordant for the inner intercrystalline crack defect of continuous casting steel billet, it is characterized in that, it is formulated by picric acid, sodium alkyl benzene sulfonate, absolute ethyl alcohol, hydrochloric acid, nitric acid, distilled water, and the chemical composition of its every part mordant proportioning is as follows:
Picric acid, i.e. trinitrophenol C
6h
3n
3o
73-4 grams
Sodium alkyl benzene sulfonate R-C
6h
4-SO
3na10-20 milliliter
Absolute ethyl alcohol C
2h
5oH, mass percent: 99.8%, 500-800 milliliters
Hydrochloric acid HCl, mass percent: 36%, 150-300 milliliters
Nitric acid HNO
3, mass percent: 63.8%,
40-60 milliliters
Distilled water 2000 milliliters.
2. adopt a kind of compound method showing the mordant of continuous casting steel billet intercrystalline crack according to claim 1, it is characterized in that,
1) quantitative picric acid solid chemicals is placed in a glass container by ormal weight, gets distilled water 2000 milliliters, be divided into two parts, portion joins in picric acid solid chemicals, and another part for subsequent use;
2) absolute ethyl alcohol getting ormal weight joins in picric acid aqueous solution, then joins in picric acid ethanol water by quantitative hydrochloric acid;
3) nitric acid separately getting ormal weight joins in distilled water for subsequent use, then mixes in aqueous solution aqueous solution of nitric acid being poured into picrate acid treatment, uniform stirring, finally quantitative sodium alkyl benzene sulfonate is poured in the solution previously prepared, abundant stirring, completes the preparation of reagent, can use.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210204195.2A CN103510092B (en) | 2012-06-20 | 2012-06-20 | Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210204195.2A CN103510092B (en) | 2012-06-20 | 2012-06-20 | Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN103510092A CN103510092A (en) | 2014-01-15 |
| CN103510092B true CN103510092B (en) | 2015-10-07 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105316685B (en) * | 2014-07-16 | 2018-02-27 | 鞍钢股份有限公司 | Cold etching agent for displaying ingot type segregation of bearing steel casting blank and preparation method thereof |
| CN106086906B (en) * | 2016-06-08 | 2019-02-12 | 中国船舶重工集团公司第七二五研究所 | It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product |
| CN108169113A (en) * | 2017-12-28 | 2018-06-15 | 江苏和兴汽车科技有限公司 | A kind of quick detection agent and its detection method |
| CN108225872A (en) * | 2018-01-29 | 2018-06-29 | 攀钢集团攀枝花钢铁研究院有限公司 | For detecting the detection method of the corrosive agent of weld seam macrostructure, preparation method and caustic solution and weld seam macrostructure |
| CN110144619B (en) * | 2019-06-05 | 2020-06-16 | 天津重型装备工程研究有限公司 | Dendritic crystal corrosive agent and corrosion method for large-ingot modified IN617 alloy |
| CN111366526A (en) * | 2020-03-27 | 2020-07-03 | 阳春新钢铁有限责任公司 | Corrosive agent for dendritic structure of 20MnSiV steel and display method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101587040A (en) * | 2009-04-30 | 2009-11-25 | 黄楠 | Macroscopic defect cold etching visualizing reagent |
| CN102401759A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Cold etching agent for ultra-low carbon steel casting blank low-magnification grain structure and preparation method thereof |
-
2012
- 2012-06-20 CN CN201210204195.2A patent/CN103510092B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101587040A (en) * | 2009-04-30 | 2009-11-25 | 黄楠 | Macroscopic defect cold etching visualizing reagent |
| CN102401759A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Cold etching agent for ultra-low carbon steel casting blank low-magnification grain structure and preparation method thereof |
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